反应详情

Carbonyldiimidazole (1.53 g, 9.41 mmol) was added to a solution of tert-butyl 4-[(2-amino-5-fluoropyridin-3-yl)amino]piperidine-1-carboxylate (0.73 g, 2.35 mmol) in acetonitrile (10 mL) at room temperature. The reaction was stirred until all the starting material was consumed (approximately 2 h) and then the solvent was evaporated in vacuo. The residue was diluted with water, extracted with dichloromethane (3×), dried over magnesium sulfate and then concentrated. The crude product was purified by chromatography (silica gel, 1% to 10% methanol in methylene chloride gradient elution), which gave the title compound (0.309 g). MS 337.2 (M+1)

1. customwas consumed (approximately 2 h)
2. customthe solvent was evaporated in vacuo
3. additionThe residue was diluted with water
4. extractionextracted with dichloromethane (3×)
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customThe crude product was purified by chromatography (silica gel, 1% to 10% methanol in methylene chloride gradient elution), which